Patent US4310663A successfully refreshed from Google Patents.
US4310663A
Expired / Lapsed
US
⏱️ 0.0 years remaining
Continuous process for producing water-soluble hydroxyalkyl cellulose and related ethers
Assignee: Hoechst AG
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Filing: 1980-06-04
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Granted: 1982-01-12
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Expires: 2000-06-04
Abstract
Abstract A continuous process for manufacturing water-soluble hydroxyalkyl cellulose, and water-soluble mixed ethers based on hydroxyalkyl cellulose, comprising producing a slurry comprising (by weight) 1 part cellulose, 0.02 to 0.6 parts alkali metal hydroxide, 5 to 10 parts inert organic solvent, and 0.4 to 2.5 parts water; continuously feeding the slurry to a first elevated pressure reactor and mixing the slurry therein with at least one normally gaseous etherifying agent which has been liquified under pressure; maintaining the slurry at a temperature up to 40° C., and a gauge pressure up to 3 bars, for 15 to 90 minutes, to give a degree of substitution from 0.2 to 1.0; continuously circulating the slurry in the first reactor in a loop through a homogenizing device to form a homogenized slurry; continuously feeding the homogenized slurry through a tubular reactor having a conveying device, an inlet, and first and second parts, and reacting the homogenized slurry in the tubular reactor for 70 to 180 minutes at a temperature from 30° to 120° C., under a gauge pressure of up to 10 bars, continuously transferring the reacted slurry into a cooling device; and subsequently purifying the etherified compounds; and apparatus for performing the process utilizing pressurized etherifying reactors and a heated tubular reactor.
Inventors
- 👤 Josef Hilbig
- 👤 Arno Holst
- 👤 Hans Kunkler
- 👤 Klaus Stolting
- 👤 Wolfgang Schminke
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-02 15:14
CPC Classifications
C; C08; C08B; C08B11/00; C08B11/02; C08B11/04; C08B11/08; C08B17/00; C08B17/06
Claims Analysis
Total Claims: 16
Claim 1
Independent Claim
260 words
A continuous process for the manufacture of water-soluble hydroxyalkyl cellulose, and water-soluble mixed ethers based on hydroxyalkyl cellulose, comprising the steps of: producing an initial slurry comprising 1 part by weight of cellulose, about 0.02 to 0.6 parts by weight of an alkali metal hydroxide, about 5 to 10 parts by weight of an inert organic solvent, and about 0.4 to 2.5 parts by weight of water; continuously feeding said initial slurry into a first apparatus suitable for operation at elevated pressure, and mixing said initial slurry therein with at least one hydroxyalkyl etherifying agent which is gaseous at atmospheric pressure and at room temperature, and which has been liquefied under pressure; maintaining said slurry in said first apparatus at a temperature of up to about 40° C., and under a gauge pressure of up to about 3 bars, for a residence time of from about 15 to 90 minutes, to give a degree of substitution in the range of from about 0.2 to about 1.0; continuously circulating said slurry in said first apparatus in a loop through a homogenizing device, to form a homogenized slurry; continuously feeding said homogenized slurry through a tubular reactor having a conveying device, an inlet, a first part, and a second part, and reacting said homogenized slurry in said reactor for a residence time of about 70 to 180 minutes at a temperature of from about 30° C. to 120° C., under a gauge pressure of up to about 10 bars; and continuously transferring the reacted slurry from said reactor into a cooling device.
Claim 2
Dependent Claim
260 words
A continuous process for the manufacture of water-soluble hydroxyalkyl cellulose, and water-soluble mixed ethers based on hydroxyalkyl cellulose, comprising the steps of: producing an initial slurry comprising 1 part by weight of cellulose, about 0.02 to 0.6 parts by weight of an alkali metal hydroxide, about 5 to 10 parts by weight of an inert organic solvent, and about 0.4 to 2.5 parts by weight of water; continuously feeding said initial slurry into a first apparatus suitable for operation at elevated pressure, and mixing said initial slurry therein with at least one hydroxyalkyl etherifying agent which is gaseous at atmospheric pressure and at room temperature, and which has been liquefied under pressure; maintaining said slurry in said first apparatus at a temperature of up to about 40° C., and under a gauge pressure of up to about 3 bars, for a residence time of from about 15 to 90 minutes, to give a degree of substitution in the range of from about 0.2 to about 1.0; continuously circulating said slurry in said first apparatus in a loop through a homogenizing device, to form a homogenized slurry; continuously feeding said homogenized slurry through a tubular reactor having a conveying device, an inlet, a first part, and a second part, and reacting said homogenized slurry in said reactor for a residence time of about 70 to 180 minutes at a temperature of from about 30° C. to 120° C., under a gauge pressure of up to about 10 bars; and continuously transferring the reacted slurry from said reactor into a cooling device.
Claim 3
Dependent Claim
24 words
A process as disclosed in claim 1, wherein said initial slurry further comprises an etherifying agent which is solid or liquid at atmospheric pressure.
Claim 4
Dependent Claim
39 words
A process as disclosed in claim 1 or 2, wherein the total proportion of etherifying agent added to the initial slurry and to the first apparatus is 0.3 to 3.2 parts by weight per part by weight of cellulose.
Claim 5
Dependent Claim
88 words
A process as disclosed in claim 1, further comprising the step of continuously feeding said homogenized slurry from said first apparatus into at least one second apparatus suitable for operation at elevated pressure, and maintaining said homogenized slurry in said second apparatus at a temperature of up to about 40° C., and under a gauge pressure of up to about 3 bars, for a residence time of from about 15 to 90 minutes, to give a degree of substitution in the range of from about 0.5 to 1.5.
Claim 6
Dependent Claim
34 words
A process as disclosed in claim 4, wherein further etherifying agent is introduced in liquid or dissolved form into the slurry in at least one of said devices suitable for operation at elevated pressure.
Claim 7
Dependent Claim
34 words
A process as disclosed in claim 4, wherein a cross-linking agent is introduced in liquid or dissolved form into the slurry in at least one of said devices suitable for operation at elevated pressure.
Claim 8
Dependent Claim
47 words
A process as disclosed in claim 1, wherein said initial slurry comprises 1 part by weight of cellulose, 0.2 to 0.4 parts by weight of an alkali metal hydroxide, 6 to 8 parts by weight of organic solvent, and 1.0 to 2.1 parts by weight of water.
Claim 9
Dependent Claim
38 words
A process as disclosed in claim 3, wherein the total proportion of etherifying agent added to the initial slurry and to the first apparatus is about 0.6 to 2.0 parts by weight per part by weight of cellulose.
Claim 10
Dependent Claim
93 words
A process as disclosed in claim 1, wherein the inlet temperature of the slurry in said tubular reactor is up to about 40° C., the temperature of the slurry is raised to up to about 60° C. in said first part of said reactor, during about 30 to 90 minutes of residence time and a temperature of about 60° C. to 120° C. is maintained in the second part of the tubular reactor during the remaining 40 to 90 minutes of residence time, under a gauge pressure of up to about 5 bars.
Claim 11
Dependent Claim
23 words
A process as disclosed in claim 1 or 9, wherein the total residence time in the tubular reactor is 90 to 140 minutes.
Claim 12
Dependent Claim
17 words
A process as disclosed in claim 1, wherein additional etherifying agent is added in said tubular reactor.
Claim 13
Dependent Claim
17 words
A process as disclosed in claim 1, wherein a cross-linking agent is added in said tubular reactor.
Claim 14
Dependent Claim
22 words
A process as disclosed in claim 1, 2, 4, or 7, wherein said etherifying agent in said first apparatus is ethylene oxide.
Claim 15
Dependent Claim
26 words
A process as disclosed in claim 2, wherein said etherifying agent in said initial slurry is monochloroacetic acid, a salt of monochloroactic acid, or propylene oxide.
Claim 16
Dependent Claim
33 words
A process as disclosed in claim 3, wherein said etherifying agents are selected such that said process produces hydroxyethyl cellulose, hydroxypropyl cellulose, hydroxyethyl-hydroxypropyl cellulose, hydroxyethyl-methyl cellulose, hydroxyethyl-hydroxypropyl-methyl cellulose, hydroxyethyl-ethyl cellulose, or hydroxyethyl-carboxymethyl cellulose.
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USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1985-01-11 | 1985-07-13 | 1986-01-12 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1989-01-11 | 1989-07-13 | 1990-01-12 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1993-01-11 | 1993-07-13 | 1994-01-12 | $7700.00 | Window Closed / Lapsed |